Method for preparing polyphenylene sulfide/graphene composite material through in situ polymerization
A technology of polyphenylene sulfide and composite materials, which is applied in the field of in-situ polymerization to prepare polyphenylene sulfide/graphene composite materials, can solve problems such as poor toughness, achieve improved thermal conductivity, simple preparation process, and expand the application range
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Embodiment 1
[0022] Step 1: Preparation of graphene-sodium sulfide monomer dispersion
[0023] 480gNa 2 S·9H 2 0, anhydrous lithium chloride 30g, anhydrous sodium acetate 15g add the polymerization reactor that contains mechanical stirring device, add the solvent N-methylpyrrolidone of 3000ml simultaneously, the graphene dispersion liquid of 2000ml (solvent is N-methylpyrrolidone, The content is 1mg / ml), fill with nitrogen, close the reactor after exhausting the air, raise the temperature to 180°C, and perform azeotropic distillation for dehydration. After removing all the water of sodium sulfide, the graphene-sodium sulfide monomer dispersion liquid that can be used for polymerization reaction is obtained.
[0024] Step 2: Polycondensation reaction
[0025] Add 294g of p-dichlorobenzene to the above reaction kettle, then add 500ml of N-methylpyrrolidone, fill the kettle with nitrogen, close the reaction kettle, raise the temperature to 220°C for 3 hours, then raise the temperature to 2...
Embodiment 2
[0029] Step 1: Preparation of graphene oxide-sodium sulfide monomer dispersion
[0030] 480gNa 2 S·9H 2 O, anhydrous lithium chloride 30g, anhydrous sodium acetate 15g add the polymerization reactor that contains mechanical stirring device, add the solvent N-methylpyrrolidone of 4000ml simultaneously, the graphene oxide dispersion liquid of 1000ml (solvent is N-methylpyrrolidone , with a content of 1.2 mg / ml), filled with nitrogen, exhausted the air, closed the reactor, raised the temperature to 180°C, and dehydrated by azeotropic distillation. After the water of sodium sulfide is completely removed, a graphene oxide-sodium sulfide monomer dispersion that can be used for polymerization is obtained.
[0031] Step 2: Polycondensation reaction
[0032] Add 294g of p-dichlorobenzene to the above reaction kettle, then add 500ml of N-methylpyrrolidone, fill the kettle with nitrogen, close the reaction kettle, raise the temperature to 220°C for 3 hours, then raise the temperature ...
Embodiment 3
[0036] Step 1: Sodium Sulfide Dehydration
[0037] 480gNa 2 S·9H 20, anhydrous lithium chloride 30g, anhydrous sodium acetate 15g add the polymerization reactor that contains mechanical stirring device, add the solvent N-methylpyrrolidone of 5000ml simultaneously, charge into nitrogen, close reactor after air is discharged, be warming up to 180 ℃, dehydration by azeotropic distillation. When the water of sodium sulfide is removed, sodium sulfide that can be used for polymerization reaction is obtained.
[0038] Step 2: Polycondensation reaction
[0039] Add 294g of p-dichlorobenzene to the above reaction kettle, then add 500ml of N-methylpyrrolidone, 1000ml of graphene oxide dispersion (the solvent is N-methylpyrrolidone, the content is 1.2mg / ml) and fill the kettle with nitrogen, Close the reactor, raise the temperature to 220°C for 3 hours, and then raise the temperature to 260°C for 3 hours. Stop the reaction, lower the temperature, and deflate to obtain a graphene oxi...
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